関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Isopropyl Acetate | HCID 7915 | — |
| 反応物 | 1,3-Dimethoxybenzene | HCID 9025 | — |
| 反応物 | Methyl 2-Bromo-5-nitrobenzoate | HCID 245494 | — |
| 反応物 | 2-Bromo-1,3-dimethoxybenzene | HCID 612296 | — |
| 反応物 | 2-Iodo-1,3-dimethoxybenzene | HCID 11391407 | — |
| 反応物 | Methyl 2-iodo-5-nitrobenzoate | HCID 11415548 | — |
| 反応物 | Methyl 5-nitro-2-{[(trifluoromethyl)sulfonyl]oxy}benzoate | HCID 18755364 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 生成物 | Methyl 5-nitro-2-(2,6-dimethoxyphenyl)-benzoate | HCID 11001627 | — |
反応手順
The process comprising treating 2-bromo-1,3-dimethoxybenzene, 2-iodo-1,3-dimethoxybenzene or 1,3-dimethoxybenzene with an organolithium reagent in a first solvent at a temperature of about −5° C. to about 15° C., preferably about 0° C. to about 5° C., after complete addition of the organolithium reagent, the temperature is allowed to warm to ambient temperature and the reaction mixture is stirred for about 1 to 4 hours, preferably about 2 hours, recooling the reaction mixture to about 0° C. and then adding ZnCl2 while maintaining the temperature between −5° C. and 15° C., preferably about −5° C. to about 5° C., after complete addition of ZnCl2 allowing the temperature to warm to ambient temperature and allowing the reaction mixture to stir for about 1 to 4 hours, preferably about 2 hours, recooling the reaction mixture to about 0° C. and adding methyl 2-bromo-5-nitrobenzoate, methyl 2-iodo-5-nitrobenzoate or methyl 5-nitro-2-{[(trifluoromethyl)sulfonyl]oxy}benzoate followed by addition of first transition metal catalyst and maintaining the reaction temperature between about 10° C. and about 55° C., preferably between about 20° C. and about 45° C., about 30 minutes after complete addition of first transition metal catalyst adding isopropylacetate and stirring for about 20 to about 90 minutes and then filtering to provide methyl 2′,6′-dimethoxy-4-nitro-1,1′-biphenyl-2-carboxylate;
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06673930B2 |
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| 出典データセット | uspto-grants-2004_01 |
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| ORD ID | ord-9b0412d15e8847f1b15689a2753da5d3 |
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| 出典メモ | uspto-grants-2004_01 |
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